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SCIENCE & METROLOGY SOLUTIONS 1 News from CAMECA François Horréard, Product manager

News from CAMECA - Start - Helmholtz-Zentrum für ... worldwide organization • CAMECA Instr. Inc Madison, WI, USA 3D Atom Probe , 67 employees • CAMECA – Headquarters Gennevilliers,

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News from CAMECA

François Horréard,Product manager

2Science & Metrology Solutions

Electronic Instruments GroupElectromechanical Group

ICP‐OES / ED‐OES / XRF

EBSD /  EDS  /  WDS  / Micro‐XRF

High Speed Digital Cameras

X‐Ray and Gamma‐Ray Detectors, Digital Pulse Processors XRF

AMT (Advanced Measurement Technologies)Radiation detectors

Stirling engines, CryocoolersEIS (Electrical Impedence

Spectroscopy)

ICP‐MS / GD‐MS / TIMS / IRMSSIMS / EPMA / APT 

(15 000 employees worldwide)

CAMECA worldwide organization

• CAMECA Instr. Inc Madison, WI, USA3D Atom Probe ,

67 employees

• CAMECA – HeadquartersGennevilliers, FranceSIMS, EPMA, LEXES

168 employees(38% R&D and engineers)

• CAMECA Germany9 employees

• Ametek India5 CAMECA employees

• CAMECA Korea13 employees

• CAMECA Japan13 employees

• CAMECA Taiwan9 employees

• Nu instrumentsWrexham, UK

ICPMS, gas, TIMS, GDMS130 employees

• R&D and industrial center• Sales and Service

• Ametek Russia1 CAMECA employee

• Ametek China5 CAMECA employees

• Ametek do Brazil1 CAMECA employee • Australia

2 CAMECA employees

3Science & Metrology Solutions

Agents in other areas

Three development & manufacturing sites

4Science & Metrology Solutions

Atom Probe Technology Center, Madison, WI, USA

CAMECA Nu Instruments, Wrexham, UKICP‐MS, TIMS, GD‐MS, Gas MS

CAMECA Headquarters, Gennevilliers, FranceSIMS, EPMA, LEXES

EPMAElectron Probe MicroAnalysis

SIMSSecondary Ion Mass Spectrometry

APTAtom Probe Tomography

World Leader in Elemental & Isotopic Microanalysis

www.cameca.com France, Brazil, China, Germany, India, Japan, Korea, Russia, Taiwan, UK, USA.

IMS Wf , SC Ultra

IMS 7f-Auto , 7f-GEO

SIMS 4550

IMS 1300-HR3 , KLEORA

NanoSIMS 50L

EIKOSTM

LEAP® 5000

EX-300

SXFive, SXFiveFE

Electrons in / X rays out Ions in / ions out E field / ions out

ICP-MSInductively Coupled PlasmaMass Spectrometry

Liquid/Solid (Laser) in(Plasma source)/ions out

SIRMSStable Isotope Ratio Mass Spectrometry

Gas in (Electron source)/ions out

TIMSThermal Ionization Mass Spectr.

Solid in (Thermal source)/ions out

Innovator in Elemental & Isotopic Mass Spectrometry

www.nu-ins.com France, Brazil, China, Germany, India, Japan, Korea, Russia, Taiwan, UK, USA.

HORIZONPERSPECTIVE

PANORAMA

NOBLESSE HR

TIMS

PLASMA 1700

PLASMA 3

ATTOM ESASTRUM

GDMSGlow Discharge Mass Spectr.

Solid in (Glow discharge source)/ions out

Noble GasNoble Gas Mass SpectrometryGas in (Electron source)/ions out

Microanalysis & bulk elemental analysis

7Science & Metrology Solutions

8Science & Metrology Solutions

3D atom probe

The New

Optimal performance UV Laser Up to 80% detector efficiency MHz pulse frequency Microtip specimen handling

Most diverse Applications Space,including Geosciences

New hardware designs Pre-aligned electrode Simplified Specimen Stage Simplified Cryo System Simplified Green Laser option

Outstanding performance at lowest Cost of Ownership

The LEAP 5000

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SCIENCE & METROLOGY SOLUTIONS

1023

nm 10

0 nm

Y

Pb

YPb Y & Pb

207Pb

206Pb

20 n

m

100

nm

20 n

m

APT of 4.4 Ga Zircon, 2014■ Analysis of the oldest

known piece of the earth by Dr. John Valley has helped to drive interest in atom probe analysis of natural geological materials

■ This work demonstrated the feasibility of isotopic analysis and aging of nanodomains in zircon

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What you will NOT see today:

10Science & Metrology Solutions

3D atom probes

The New in live demonstration at M&M conference,6-10 Aug. 2017, St Louis, MI, USA

Product Launch during Goldschmidt

11Science & Metrology Solutions

From the Plasma 3 MC ICPMS…

Collision/Reaction cell Multi‐collector ICP‐MSThe new

Why add a Collision/Reaction cell ?

The Argon ICP ion source produces a significant beam of Ar+ ions (~10’s μA) alongwith polyatomic molecules such as ArH, Ar2+ and ArO+

These can interfere directly with the atomic ions of the same nominal mass forexample K, Fe

Polyatomic interferences are currently dealt with using the high resolutioncapabilities of MC-ICP mass spectrometers but with some limitations (transmission)

Analysis of elements such as Ca is difficult on current multi-collectors due to thepresence of the large argon beam

The ion current from Ar+ ions also affects the abundance sensitivity of higher massions

1228 August 2017

Benefits of Collision/Reaction cell ?

Hydrogen Collision gas Argon ions undergo a charge exchange with hydrogen

Ar+ + H2 Ar + H2+ ArH+ + H2 Ar + H3+ ArO+ + H2 Ar + H2O+

This can reduce the Argon ion signal by > 9 orders of magnitude while other analytes are unaffected.

Oxygen or Ammonia Collision gas Interferences can be shifted in mass

M+ + O2 MO+ + O M+ + NH3 MNH3+

1328 August 2017

The technical solution: a dual path

Dual path does not require cell gas to be stopped

High energy beam does not pass through RF multipoles and behaves exactly as the Plasma 3

1428 August 2017

COLLISION/REACTIONCELL

TRANSFER OPTICS TO MASS ANALYZERSOURCE

Low Energy Path with Collision/Reaction cell for interference removal High energy Path for classical Multi-Collector performance Up to 4 independently controlled reaction gas inlets Shipment of the first instrument to Harvard in Q3 2017 (K and Ca

isotopes for cosmo-chemistry applications).

28 August 2017 15

Summary

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Mid-2016: Introducing the IMS 1300-HR3

IMS 1300-HR3

High ReproducibilityHigh Spatial ResolutionHigh Mass Resolution

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■ High brightness RF-plasma oxygen ion source■ Automated sample loading system■ Motorized sample height (Z) adjustment■ UV-light microscope■ Low noise 1 E12 Ω resistor Faraday cup preamplifier boards■ Pfeiffer turbo-molecular pumps■ Updated Electronics & Software

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Mid-2017: testing the IMS 1300-HR3 before shipment in Sept. to JAEA

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Preparing the opening of a showroom at CAMECA

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Finishing the installation of an EPMA SX Five FE, an IMS 7f-Auto and a NanoSIMS 50L.

The NS50L will be operated from a separate control room.

THERMO water chiller (water-water) and ERKOM air compressor (8bars) in the same room.

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CAMECA Organization & new personnel

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Jean-Charles Chen, CAMECA BU manager

SIMS Sales, academic

Philippe Saliot

Dr. Etienne Wortham, Service Business

Patrick McCarthy, Global OPEX Director + acting Global Service Manager

R&D and Product MarketingDr. Michel Schuhmacher

(Dr. Laurent Roussel)

Jean-Charles Chen,Acting VP Sales & Service

Claude Guignes,Services Operation

Mathias Carrachioli,FSE manager France

Dr. Ulrich Erkhe,Service manager, Cameca Ger.

Dr. Wolfgang Berneike,Country manager, Cameca Ger.

Subsidiaries(sales & service)

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CAMECA Organization & new personnel

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R&D and Product MarketingDr. Michel Schuhmacher

(Dr. Laurent Roussel)

Product Marketing

Dr. Dave Larson manages the technical product mgrs:- Dr. Paula Peres: IMS 7f, IMS 1300- Dr. Olivier Dulac: LEXES, IMS Wf & SCU- Dr. Anne-Sophie Robbes: SX 5 EPMA - Dr. Rob Ulfig: EIKOS APT- Dr. David Reinhardt: LEAP APT- François Horréard: NanoSIMSEach PM manages the corresponding App. Lab

CAMECA searching (again) for a NS50 application lab manager !

R&D

- François Hillion: adjunct R&D mgr& NanoSIMS project leader

- Dr. Nicolas Saquet, ion sources

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A new RF-plasma O- primary ion source

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NS50L equiped with RF plasma

RF plasma O- primary ion source

Rack for electronics & cooler

Oxygen gas inlet

Cs+ Source chamber

Cooling

Wien mass filter

Mechanical interface

Photos by courtesy of Pr. M. Kilburn, UWA, Perth, Australia.

Similar performance between the new RF-plasma ion source in O- mode and the CAMECA microbeam Cs+ ion source.

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U Particles with RF plasma O- ion source

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Linear scale

LOG scale

Elements Field of View, µm Nb pixels Dwell,

ms/pix/cycle Cycles Total acq time Primary beam current (pA)

250.577 5 x 5 256 x 256 4 1 4m 41s 3

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U Particles with RF plasma O- ion source

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0.00 0.50 1.00 1.50 2.00 2.50 3.00

Distance µm

0

50

100

150

200

250

300

Co

unts

238U

0.00 0.50 1.00 1.50

Distance µm

0

50

100

150

200

250

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Counts

238U

16-84%: ~125 nm, 16keV O-, 3 pA

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Improved in-situ optical microscope & LED illumination

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2052 x 2456 pixel digital camera

Fixed 700µm FOV

Digital zoom: no mechanical shift when zooming.

Homogeneous white LED illumination over the FOV.

1.5 µm lateral resolution

Digital zoom700 µm FOV

Zircon grains, 700 µm FOV

50µm

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Magnetic transfer rods

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NanoSIMS control software: the current version is V 4.4

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2 x 2 µm direct profiles

2 x 2 µm crater after depth profile

The NanoSIMS permits depth profiling from a few µm2 areas with unique sensitivity

For µm-size structures with high aspect ratio, direct profiles can be faster than profile reconstruction from ROIs

Sample drift can become a limitation

1H

12C

16O

19F

27NanoSIMS

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Alternated Drift correction

To be tested hopefully for SIMS XXI…

Alternated drift correction for very small direct depth profiles or image stacks without contrast : - Recording image #1 of a small detail present in the largest FoVaccessible, before starting acquisition (SEM, TIC, SIMS),- Start image stack or direct depth profile acquisition,- After a preset cycle nb, automated pause, de-zoom, zoom on the smalldetail, record and save the image #2,- Compare images i and i+1, apply drift correction, correct beamposition with electrostatic deflection,- Restart image stack or profile,Etc…

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WinImage II: version 4.4

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Switch to Windows (7 & 10) 64 bits: better handling of large image stacks

Copy-Paste of images: in EMF (vectorial format keeping texts sharp) Without border (for mosaics) With 0, 1 or 2 lines of infos below the images

Import of external images (SEM, TEM, optical, …) , streching, rotation, scaling and matching SIMS-External or External -SIMS.

Superimposition of 3D images in RGB (red green blue)

Image filtering (= smoothing: Gaussian, Median, Box)

Display of profiles from multiple ROIs and line-scans from multiple cycles: ergonomy, saveable symbols & colors, flexibility

Reduction of stacks: pixel summing, cycle summing, cycle suppressions

Cycle automatic scan allowing 3D movies recording

Caliper: distance measurement on images

Corrections of many former Pbs

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Import external images (BSE, SEM, ….)

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Automated strech and superimposition of external image(2, 3 or 4 alignment points)

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SIMS ImportedSEM

Streched & Alignedimported SEM

Images by courtesy of Motoo Ito, JAMSTEC

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WinImage II, Multi ROI Depth Profiles

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3D display

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volume

isosurface

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3D view in RGB superimposition

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WinImage II, Scatter Plot

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WinImage II, Automated ROI definition

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WinImage II, file manager

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Website: www.cameca.com

Scientific articles

38NanoSIMS

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Thank you for your attention !

We have in the room today:

Dr. Wolfgang Berneike, General manager CAMECA GermanyDr. Ulrich Erkhe, Service manager, CAMECA Germany

Mr. Patrick Mc Carthy, Global OPEX Director & acting Global Service Manager

Dr. Etienne Wortham, Service Business

Mr. François Hillion, NanoSIMS project leader

Mr. François Horréard, NanoSIMS product manager